Sampling apparatus



Feb, 6, 1951 s. L. HANDFORTH '2,540,944

' SAMPLING APPARATUS Filed July 2l, 1945 2 Sheets-Sheet l Feb- 6, 1951 s. L.. HANDFORTH 2,540,944

SAMPLING APPARATUS Filed July 21, 1945 2 sheets-sheet 2 F15. E. F154.

flue/jg 5L A h i IJI /f if 5 7 j y 6 I l /fl Ask y 8 -f t 53@ zj*- Patented Feb. 6, 1 951 SAMPLING APPARATUS Stanley L. Handforth, Wilmington, Del., assigner to the United States oi America as represented by the United States Atomic Energy Commission Application July 21, 1945, Serial No. 606,402

(Ci. 'i3- 422) 7 Claims.

The present invention relates generally to sampling apparatus and has particular relation to apparatus and methods for obtaining representative samples from relatively large bodies of radioactive or other liquids inherently dangerous to handle.

In carrying out certain chemical reaction procedures, such as the concentration of radioactive, metallic isotopes, the most suitable method f determining the progress of the reaction is by periodic, direct examination of a sample of the reacting material, and frequently this examination involves a check of its radioactive properties by the use of radiaton counters. However, despite the need therefor the obtaining of a suitable representative sample from a large body of radioactive, reacting liquid has proven a very dioult problem. Conventional sampling methods are unsatisfactory, chiefly because of the risk of serious injury to personnel which accompanies exposure to the high density radiations emanating from the main body of the reacting liquid, and the various suggested procedures, some of which involved rather complicated apparatus, have proven unreliable or otherwise unsatisfactory.

Hence the principal object of the present invention is to provide a sampling apparatus and method, particularly adapted for use in connection with processes involving large bodies of radioactive liquids, which will make available small, representative samples of the body of liquid, as such samples may be required, and which will make possible the obtaining and handling of such samples without risk of injury to the operating personnel. A further object of the invention is to provide sampling apparatus in accordance with vthe above stated principal object which shall be `simple in design, reliable and easy to operate, and suiiiciently foolproof that it will rarely if ever become inoperative.

Other objects as Well as the features of the apparatus, the various novel structural arrangements and combinations utilized therein, and the details of the method, which I have discovered, will be made more apparent by reference to the accompanying drawings and the following description of a preferred embodiment thereof. In the drawings,

Fig. 1 is a side, elevational view, partially in section, of a reaction tank provided with a sampling apparatus in accordance with this invention;

Fig. 2 is a plan View of the structure shown in Fig. 1;

L Figs.` 3 and 4 are enlarged sectional views of the sampling apparatus, taken on the general lines 3--3 and 4 4 of Fig. 2, and

Figure 5 is a plan sectional View taken along the line 5--5 of Figure 3.

The apparatus illustrated in the drawings includes a reaction tank 2 of relatively large volume for containing the reacting liquid. The tank 2 is provided with inlet and outlet piping 2a and 2b for the reacting liquid and with a central., flanged access iitting 2c for the sampling apparatus, which is indicated generally at I. Except for the openings provided by the piping 2a and 2b and the access fitting 2c, the tank 2 is completely closed. In view of the fact that highly radioactive materials will normally be contained therein, the tank 2 is either sunk in the ground, as illustrated, or it is enclosed in a radiation shield, preferably of massive, cast, concrete construction several feet thick.

The sampling apparatus I is located above the the top of the tank 2 and through the shield 3 to the bottom ofthe sampling apparatus I is provided by means of suitable pipe sections E and 4a.

The various structural elements of the sampling apparatus are enclosed within a generally cylindrical radiation shield 5 which is adapted to rest on a circular, metallic plate 5a embedded in the shield 3. The shield 5 is open at its lower end and is held in proper position relative to the support plate 5o and to the other elements of the apparatus by means of an upstanding tubular guide or baille 5b which is of somewhat larger diameter than the shield proper. To obviate any possibility of radiation leakage, the space between the main shield 5 and the guide 5b is filled with lead wool or other packing capable of shielding against radiation as illustrated at 5c. In aparticularly satisfactory embodiment of the invention, the shield 5 is made of lead with side walls approximately two inches thick, the entire shield 5 having an overall length of about 24 inches and an internal diameter of about 5 inches.

The upper end of the shield 5 is provided with a hollow boss 5d which is positioned slightly ofi center and which is adapted to be closed by a removable lead cover 5e. Two spaced passageways 5f and 5g extend from the interior of the hollow boss 5d through the top wall of the shield 5 into the interior of the shield. An air inlet conduit I3 extends through the passageway 5f and a sampling tube I5 which connects at its lower end with a. cuplike sample container Il extends through the other passageway 5g. Lead Wool is packed in the space between the walls of the passageways 5f and 5g and the members extending therethrough to prevent radiation leakage into the interior of the boss 5d.

During the'oper'ation of the apparatus, liquid is drawn into hollow interior l la of the sample container Il by means of a steam jet aspirator 8,]

and the sample container I I may berconveniently supported upon the aspirator by means such as the short circuit 8a Vwhich serves the further function of connecting the interior ila of the sample container with the low-'pressure por-tionrof the aspirator. The inlet end of the aspirator 8 is connected to a suitable steam inlet line 6 through a valve l having an operating handle i2 which is conducted through the shield and` the boss 5d by a Vsuitable opening iZa formed therein. Ther outlet=end ,of thev aspirator ii is connected to the interior of the reaction. tank 2A -bysuitable piping di.. and` preferably terminates above the normal liquid level that tank. The piping: 9is1welded orr otherwise affixed to a cap member" lib-fat lthc-:upper end of the pipe section avand serves as the main: support fortheraspiratorliandthe sample'container 'i l.

Anv updra'ft; conduit dit extends from the in .terior HaL ofthe sample Icontainer ii' toa. point below the. normal liquid level in the reaction -tankythenupper' end" of thel conduit H3 connecting Withrtheinlet. passageway 'l'a providedrin the wallsofft'heisample containerl-l. A small quan'm .tityfofrthe liquid which is .drawn through the .updzfaft conduit lil during the operationfoi .the sampling apparatus willI bei retained in4 the space I fl'a within-.the container. dueto'the fact that' the connection between the aspirator 31 and: the sample: container Ill provided' by the'conduita is"raisediaboue"tlfier bottom of the `spacel Hc in the-container; Any excess liquid moved intol the space-Ha-will overflow into the aspiratorandlie returncdto* the .maini body` of liquid in' the reaction tank .2; Theioperation of the sampling apparatusf thus efect'sf continuousv sampling of the contentsiof 'the` reaction tank 2 and `at the same time, since the inlet and overflow outlet openings inrthe vsample container H arespaced:` apartsome distance4 and? the entire operation is' accom'- panied by' intermittent turbulence', through in termiX-ing1 `of the liquid'retained inf the sample containerV `Hrand the incoming` liquid w-ill con .tinuouslp exertanieffect upony the iiquidretained. Thisiassuresathat-the sample retained? in'tlie sample-r container Virl.V shall yloeV laccuratelyrepresenta@ tive of.' they contents: of: the reaction tank 2 at any particular insta/nt.

Since' thea-spiratcr operates onithei vacuum principle;4 it.- is necessaryi that the samplingY tube p i5Y through which'` samples are removed from the sample cpntainer is" shallbe closedi during the sample fobtaining,1operation. To? accomplish.` this, .the upper end'xo'f thesamplingv tube l' isnimed with" a' conical bore, andl a removable', sonic-ally shapedsealingplug it: is provided fcirengaging this bore ,seras-'nto provide a substantial. gagtight seaif at thefupper `endl ci.' the y-samplingtube iii...

When it iszedesired to removena sample from .ther sample container it, the' aspiratcun 8; isishut .oi`f-,l the'removable1 cover- 5e is removedxthe coni'- callyV ,shapedy sealing plugi for the sampling' 'tube' If removed and?. a suitablecapillary .pipettepi not@ shown, is insertedinto`r the sample container' 'lily through' *the* sampling` tube |53;

whereupon the liquid entrapped in the container may be Withdrawn. If the radioactive material is then in a highly radioactive state, it is desirable that these operations be carried out at arms length in order to minimize risk of injury to the operator. It will be apparent that this arrangement thus` makes possible the convenient obtainingy of a small represen'tative,r sample of constant volume at any particular time in the operation of the complete apparatus.

In certain instances, it may be found necessary to locate the sampling apparatus at a consider-Y able distance: from the reaction tank 2. When this is done, difculty may be experienced in obtaining :continuous vmovement of liquid from the reaction tank 2 into the sample container 8 due to the well-known lift limitations of jet type aspirators. To overcome this difficulty, it has been found highly advantageous to provide means for admitting air to the updraft conduit l@ through -Whieh'liquid is moved` freni thefreaction. -tank 2i into the sample container I I. This meansl may `conveniently comprisev the air inlet conduit t3- which comprises ai lengthof. pipe of relatively small diameter whichisprovidedV with an orifice plug ifi at its upper end: which is open ter the atmosphere, andi whichconnects at its lower end withfthe updraft conduit -I 0 a` short distance above the liquid level in the reactiontank. By properV correlation ofthe size: of the orifice within the-orifice plug l-llwith the dimensions and pressures encountered. in. thev other.

parts .of the apparatus, the liquid moving up-f wardy in the updraft conduitY Ifll willbel broken up into small slugs interspersed by bubbles of air, and1 this arrangement will considerably increase the distance over which the. liquid can be raised without yusing excessively low pressures iny the aspirator Si. The arrangementl has; the further advantagev that increased turbulence. is produced within the sample container Il with resultant better intermixing Vofthe. contents of that container with the incoming liquid.A

When the reacting liquid is corrosive in.T natuiai-tfwill bel found highlyrdesirablefto manufacture the parts of the apparatuscontactedbyfsuch liquid. of stainless steel or other resistant ma terials.Y articula-rly good results have beerr obw tained by the use -ofa stainless steel comprising 223:percentnickelrand` l2 per centohromium, thesteel being stabilized with .Acolumbium.

Inr the particular `embodiment ofthe apparatus previously referred toA the.v down pipe 9 fromfthe jet aspirator il4 had an internal diameter =of0z65 inch;` theupdraft conduit I- hadz-an internal diameter of: about 0,25 inch; the sample container was designed to retainv approximately 1)V c.-c. `of liquid therein; the air inlet pipe t3 had an inter-nal diameterof about 0=l25 inch; and the oriilce at the inlet end offthe pipei13- had'a dameter oi approxirnatels7 0.02 inch. It 'will' be understood that theseI dimensions canv be'Y varied to satisfyl the particular requirements; of-i any g-iven-v installation, andv that' the capacity of the sample .container il 4may likewise be varied as required'.

Thesamplingapparatus' described above-con.- stitutes a simple and easily operated* means.; for obtaining representative vsamples from 'a reaction .tamper the* like, containing a large quantity ci au inherently dangerous-liquid. The; apparatus is continuous and automatic in operation, and while it -i'sA particularly designed for the'v obtaining of samples or radioactive liquids, itwili be evident thatY its use; is not' connned to'V such materials. The features of the apparatus and the improved sampling method of the invention are expressly pointed out in the accompanying claims.

What is claimed is:

1. In combination, a reaction tank adapted to contain a quantity of liquid, and means for obtaining a representative sample oi' the liquid contained in said reaction tank comprising a cuplike sample container, a conduit extending from said sample container into the liquid contained in said tank, and means connected to the sample container including an aspirator and a conduit connected thereto which discharges into said reaction tank, operable continuously to move liquid from said reaction tank through said conduit into said sample container and to return the overflow from said container to said reaction tank.

2. In combination, a reaction, tank adapted to contain a quantity of liquid, and means for obtaining a representative sample of the liquid contained in said reaction tank comprising a cuplike sample container supported above said reaction tank, a conduit extending downwardly from said sample container into the liquid contained in said tank, and a stream jet aspirator and a conduit connected thereto discharging into said reaction tank and operable continuously t0 raise liquid from said reaction tank through said conduit into said sample container and to return the overow from said container to said reaction tank.

3. In combination, a reaction tank adapted to contain a body of liquid, and means for obtaining a representative sample of the liquid contained in said reaction tank comprising a cuplike sample container of predetermined, limited capacity, conduit means extending from the interior of said container intothe liquid contained in said tank, means connected to the sample container, including an aspirator and a conduit connected thereto which discharges into said tank, operable to create a pressure diierential between the interior of said sample container and the body of liquid contained in said tank whereby liquid will be moved through said conduit into said container, means for admitting small quantities of air to said conduit to break up the liquid moved therethrough into small slugs which are spaced apart by air bubbles, and means for conducting any overiiow from said container into said aspirator whereby it will be returned to the body of liquid in said tank.

4. In combination, a reaction tank adapted to contain a body of liquid, and means for obtainduit connecting with one of said openings and extending downwardly from said container into the liquid contained in said tank, a steam jet aspirator connected to the other opening in said container and a conduit adapted to discharge the aspirator into said tank, said aspirator being operable to raise liquid from said tank through said conduit into said sample container and to return the overiiow from said container to said tank, and means including a conduit closed at one end by an orifice plug and connected at the other end to said conduit means, intermediate the ends thereof, for admitting air to saidconduit means to break up the liquid moved therethrough into small slugs spaced apart by air bubbles.

5. Liquid sampler apparatus comprising, in combination, a sealed sample chamber, an updraft conduit connected to the sample chamber at a level above the bottom thereof, an overflow conduit in the sample chamber at a level above the bottom thereof, exhaust means in communication with the overflow conduit, and an air inlet to the updraft conduit at a level below the sample chamber, whereby the bottom of the sample chamber continuously contains a sample of xed amount corresponding to the instantaneous condition of the liquid being sampled.

6. The apparatus of claim 5 wherein the updraft conduit connection and the overow conduit are in diametrically opposed portions of the wall of the sample chamber.

7. Liquid sampler apparatus comprising, in combination, a sealed sample chamber, an updraft conduit connected to the sample chamber, a vertical uid ow conduit including an aspirator portion adjacent to the sample chamber, a horizontal conduit connected between said aspirator portion and the sample chamber at a level above the bottom of the sample chamber, and an air inlet to the updraft conduit at a level below the sample chamber, whereby the bottom of the sample chamber continuously contains a sample of iixed amount corresponding to the instantaneous condition of the liquid being sampled.

STANLEY L. HANDFORTH.

REFERENCES CITED The following references are of record in the file of this patent:

UNITED STATES PATENTS Number Name Date 330,366 Arthur Nov. 17, 1885 364,512 Harrison June '7, 1887 2,225,798 Price Dec. 24, 1940 2,350,323 Cochran et al. I June 6, 1944 2,386,282 Watson et al. Oct. 9, 1945 

